反应详情

In an ice-bath thionyl chloride (39.5 ml, excess) was slowly added to [1-(3,4-dichloro-phenyl)-1H-imidazol-4-yl]-methanol (9.6 g, 39.5 mmol). The resulting mixture was stirred for 24 h. After evaporation, the oily residue was triturated with ether and 10.12 g (86%) of the hydrochloride salt of the title compound was obtained as an off-white solid. To obtain the free base, the salt was carefully neutralized with aqueous NaOH (2N) and extracted with AcOEt. The organic phase was dried (Na2SO4) and concentrated to obtain 8.43 g (95%) of the title compound as an off-white solid. Mp. 146-147° C. dec. (AcOEt/hexane), MS: m/e=260 (M+)

1. customAfter evaporation
2. customthe oily residue was triturated with ether and 10.12 g (86%) of the hydrochloride salt of the title compound
3. customwas obtained as an off-white solid
4. customTo obtain the free base
5. extractionextracted with AcOEt
6. dry with materialThe organic phase was dried (Na2SO4)
7. concentrationconcentrated